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Fly Ash Polymer Concretes

Conference Paper · June 2010

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Lech Czarnecki Andrzej Garbacz

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Coventry University and
The University of Wisconsin Milwaukee Centre for By products Utilization
Second International Conference on Sustainable Construction Materials and Technologies
June 28 June 30, 2010, Università Politecnica delle Marche, Ancona, Italy.
Proceedings of Honouree sessions ed. T Naik, F Canpolat, P Claisse, E Ganjian,
ISBN 978 1 4507 1487 7 http://www.claisse.info/Proceedings.htm

Fly Ash Polymer Concretes

Lech Czarnecki, Andrzej Garbacz, and Joanna J. Sokołowska

Department of Building Materials Engineering, Faculty of Civil Engineering of Warsaw

University of Technology – Al. Armii Ludowej 16, 00-637 Warsaw, Poland. E-mail:
<[email protected]>, <[email protected]>, <[email protected]>.

ABSTRACT

In the paper the effect of silica microfiller replacement by calcium fly ashes on polymer
concrete mechanical properties, as well as binder hardening characteristics were investigated.
This approach follows the sustainable development requirements in a building industry.
Additionally, replacing components with less expensive equivalents lowers the material cost.
Although fly ashes are commonly used in portland cement concrete technology, the calcium
fly ashes are difficult to utilize in CC, mainly due to high variation in chemical composition.
Investigation was carried out for polyester resin and calcium fly ashes from brown and hard
coal combustion, with special attention given to the second one, as fly ash of lignite showed
substantial similarities in properties to silica microfiller – quartzite meal. Twenty mixes with
different polymer/microfiller, aggregate/polymer and microfiller/aggregate ratios were tested
using statistical design of experiment. The obtained results were used for optimization of
composition of PC containing calcium fly ash.

INTRODUCTION

FC – polymer concrete, the concrete-like composite where portland cement binder is

substituted with an organic resin [Czarnecki 2005] is considered as a high performance
material due to its main advantages – high values of mechanical parameters and chemical
resistance. Those demanded in civil engineering features cause that the range of application
of PC is wide [Fowler 1999, Czarnecki 2007] – e.g. pre-cast elements, such us manholes,
sewer pipes, drainage channels, chemically resistant vessels and anti-corrosion protection of
various structures that stay in contact with chemically aggressive agents, e.g. industrial floors
[Ohama 2004, Czarnecki 2005]. Good mechanical strength, as well as chemical resistance,
are obtained in PC thanks to specific properties of high quality components. High material
cost of PC is the main drawback against the common use of this composite.

One of the methods of lowering the material cost is replacing components with not so
expensive equivalents but the substitution should be still accompanied by fulfilling the
material and technical requirements. The equivalents do not need to be raw substances, as
recently – in accordance with the precepts of sustainable development – a lot of effort is done
to utilize wastes and by-products in civil industry (also in polymer concretes technology
[Bignozzi et al. 2004, Choi et al. 2001, Lancellotti 2000]). Such approach is well known from
cement concrete technology where a number of various mineral additives is used and one of
the commonly used additives is fly ash. However, some kinds of fly ashes are difficult to
 utilize in cement concrete technology, mainly due to high variation of their chemical
composition.

In this paper the effect of silica microfiller replacement by calcium fly ashes on selected
polyester concrete mechanical properties (compressive, flexural and tensile strength), as well
as binder hardening characteristics were investigated. The range of silica microfiller
replacement by calcium fly ash was discussed. The investigation was carried out for two
types of calcium fly ashes, the by-products from hard coal and brown coal (lignite)
combustion.

CHARACTERISTICS OF APPLIED CALCIUM FLY ASHES

Both calcium fly ashes applied in the polyester concrete in this investigation were the by-
products of energetic industry. They were the by-products of coal combustion that took place
in Polish power stations. The first fly ash was the by-product of the hard coal combustion in
cogeneration placed in Warsaw and the second type was the by-product of the lignite
(referred also as brown coal) combustion in power station placed in central Poland.

The granulation of applied microfillers – the calcium fly ashes, as well as the quartzite meal –
was tested using the laser granulometer Horiba L300 (Fig.1). .

a) b)
120,000
QM
HC
100,000
BC
20,000

80,000
Q, [%]
q, [%]

60,000

10,000
40,000

20,000 QM
HC
BC
0,000 0,000
0,100 1,000 10,000 100,000 1000,000 0,100 1,000 10,000 100,000 1000,000
Diameter, [μm] Diameter, [μm]

Fig. 1. Grain Size Distribution Curves for Quartzite Meal (QM), Calcium Fly
Ash of Hard Coal (HC) and Calcium Fly Ash of Brown Coal (BC): a – Relative
Frequency Plot; b – Cumulative Frequency Plot

The results of the tests showed that the considered calcium fly ashes contained more fraction
of grain size below 1 μm. The size of the particles of fly ash of hard coal as well as quartzite
meal did not exceed 75 μm but the fly ash of brown coal contained fraction 100 μm.

EFFECT OF CALCIUM FLY ASH ON POLYESTER RESIN HARDENING

The mechanical parameters of PC except the quality of the components depend also on the
aggregate to resin binder ratio as well as microfiller content [Czarnecki 1982]. The basic aim
of the research was to investigate the influence of the calcium fly ashes on the unsaturated
 polyester resin hardening process. The investigation was carried out for the specimens of
polyester resin containing various amounts of calcium fly ashes (microfiller/resin ratio: 0.25,
0.50, 0.75, 1.00) from hard and brown coal in comparison to typical microfiller – quartzite
meal. The characteristic of resin setting were determined on the basis of the measurements of
changes of temperature, viscosity and conductivity during hardening. The investigation of
setting was carried with commercial Gelnorm test system that gives possibility to automatic
test of the changes of temperature, viscosity and conductivity, simultaneously.

The obtained results of investigation of polyester resin setting with different content of
microfillers. It was noted that in case of quartzite meal (QM) and calcium fly ash from brown
coal (BC) the drop of temperature of hardening was more rapid along with increase of gel
time, whereas in case of calcium fly ash from hard coal (HC) drop of temperature of
hardening was comparable but along with much wider range of variability of gel time (see
Fig.2a). Above conclusions are repeated for relation: temperature of hardening – hardening
time, as the relation hardening time – gel time characterized by high values of correlation
ratio, r (see Fig.2b). It was observed (Fig.3) that the relative content of microfiller has
significant influence on setting of resin: the more microfiller the binder contained, the lower
the hardening temperature, the longer gel and hardening times and the lower the value of
maximal relative conductivity were. Although the applied microfillers presented differences
in granulometric composition the silica microfiller – quartzite meal – and calcium fly ash of
brown coal showed similar influence on hardening process of polyester resin, while calcium
fly ash of hard coal showed different influence. The same relative content of calcium fly ash
of hard coal caused greater decrease of temperature of hardening and greater elongation of
gel time and hardening time than quartzite meal or calcium fly ash of brown coal. Also in
case of fly ash of hard coal the distinct influence on conductivity was observed. When the
relative content exceeded value 0.75 the relative conductivity gained only 30%, what
corresponded with low workability in comparison to other mixes.

50
a)
150
b)
r = 0,99
125 40
r =0,94
r = 0,97
100
th, [min]

r = 0,93
30
T, [˚C]

r = 0,93
75

20
50 r = 0,96

10
25
HC BC QM HC BC HC

0 0
0 5 10 15 20 25 0 5 10 15 20 25
tg, [min] tg, [min]

Fig. 2. Summary Plots For Quartzite Meal (QM), Calcium Fly Ash of Hard Coal
(HC) and Calcium Fly Ash of Brown Coal (BC): a – Temperature; b – Hardening
Time; Both in Function of Gel Time
 a)
150 r = 0,98
b) r = 0,99

125 r = 0,95 20
r = 0,96

r = 0,98
100

tg, [min]
r = 0,98
T, [˚C]

75

10
50

25
HC BC QM HC BC QM

0 0
0 0,25 0,5 0,75 1 0 0,25 0,5 0,75 1

Microfiller / Resin Microfiller / Resin

50 ratio ratio
c)
r = 0,99

40

30 r = 0,87
th, [min]

r = 0,90
20 Fig. 3. Summary Plots For Quartzite
Meal (QM), Calcium Fly Ash of Hard
10 Coal (HC) and Calcium Fly Ash of
Brown Coal (BC): a – Temperature, b
HC BC QM

0
0 0,25 0,5 0,75 1
– Gel Time, c – Hardening Time; All in
Microfiller / Resin Function of Microfiller Content
ratio

MATERIAL MODEL OF THE FLY ASH POLYMER CONCRETE

Material model assumption

The material model is defined in the form of the quadratic regression functions, in which the
amounts of the particular components are the input variables, and the technical properties are
the output variables [Czarnecki et al. 1999]:

Y = a0 + a1X1 + a2X2 + a3X3 + a11X12 + a22X22 +a33X32 + a12X12 + a13X12 + a23X23 (1)

where Y is a value of selected technical property; a0 , ..., aij are the regression coefficients;
X1 , ..., Xij are the coded material variables; Xij = Xi · Xj – mix variables.

Material variables (the real values) are transformed into coded values according to the
formula (2) which enables to use the statistic plan of experiment.

xreal = xcod · ½ · Δx + x0 (2)

where xcod is a coded variable, xreal is a real variable, x0 is a center value of range of parameter
variability and Δx is range. The variables range is a area of experiment for particular
property. For a coded variable the range is <-1; 1>.
Material model of fly ash

The preliminary tests of compressive and flexural strength for three types of polyester
mortars - containing different microfillers: quartzite meal, calcium fly ash of brown coal and
calcium fly ash of hard coal showed no significant differences in tested mechanical properties
(Fig.4).

a) b)
40 120 114.0 114.5

Compressive strength [MPa]

34.3 34.0 33.7 35.3 106.3 110.1
Flexural strength [MPa]

100.0
100 92.1
28.6 28.8
30
80
20 60
40
10
20
0 0
6.0 7.5 6.0 7.5
A/B A/B
QM BC HC QM BC HC

Fig. 4. Mechanical Parameters of Polyester Mortars Containing Quartzite

Meal (QM), Calcium Fly Ash of Hard Coal (HC) and Calcium Fly Ash of
Brown Coal (BC) in Function of A/B: a – Flexural Strength; b – Compressive
Strength

Considering the above results as well as the hardening process characteristics it was decided
to investigate the effect of replacement the quartzite microfiller with calcium fly ash from
hard coal. The basis for the determination of the material model of fly ash polymer concrete
were the results of the laboratory tests carried out using statistical design (Box compositional
design) of the experiment [Clifton et al. 1995]. An unsaturated polyester resin was used as a
binder. Aggregate consisted of standard sand and natural gravel; microfiller was the mix of
quartzite meal and calcium fly ash from hard coal combustion. The material variables were:
aggregate/binder ratio (X1, g/g), binder/microfiller ratio (X2, g/g) and calcium fly
ash/microfiller ratio (X3, g/g). The considered properties were: flexural strength (f b, MPa),
tensile strength (ft, MPa), compressive strength (fc, MPa) and density (d, kg/m3). Using the
data from the tests (Tab.1) the material model of polyester concrete containing calcium fly
ash was defined (Tab.2). Examples of graphic representation of the defined material model
of polyester PC are presented in Fig. 5.

The correlation ratios (R) higher than 0.95 and the determination ratios (R2) higher than 0.90.
indicate that the model is close to the empiric data from laboratory tests and that the
variability of PC property is strongly dependent on variability of the input variables.

ADVANCED MATERIAL MODEL – OVERALL DESIRABILITY

As polymer concrete is a composite material where various demands need to be fulfilled

simultaneously it should be evaluated according to various criteria at the same time. To make
such estimation possible the overall desirability function, developed by Harrington (1965)
was used. Three sets of evaluation criteria (wages and sufficient ranges) have been chosen
(Tab.3) and the it was evaluated whether material can be applied in the particular situations.
In all variants physical property – density is considered and its wage is always 0,10. Density
was considered as it is demanded that produced polymer concrete were possibly light. When
considering mechanical parameters only flexural and compressive strength were considered,
as the tensile strength is correlated with flexural strength. In the first variant both mechanical
properties were equivalent – their wages were equal (0.45).

Table 1. Results of Tests for Polyester Concrete with Calcium Fly Ash of Hard
Coal

Material variables Technical property

No. Flexural Tensile Compress.
Density,
A/B B/M Ash/M strength, strength, strength,
kg/m3 MPa MPa MPa
1 -0.58 -0.58 -0.58 2167 22.2 8.4 114.5
2 0.58 -0.58 -0.58 2187 20.7 10.8 102.4
3 -0.58 0.58 -0.58 2193 19.6 7.5 105.0
4 -0.58 -0.58 0.58 1746 1.7 1.7 10.7
5 0.58 0.58 -0.58 2278 20.7 10.6 113.8
6 0.58 -0.58 0.58 1854 1.9 0.6 8.6
7 -0.58 0.58 0.58 2062 17.5 7.4 70.9
8 0.58 0.58 0.58 2028 8.2 4.7 23.3
9 -0.97 0.00 0.00 2074 20.6 11.1 115.1
10 0.97 0.00 0.00 2121 11.6 7.2 40.8
11 0.00 -0.97 0.00 1961 3.2 2.8 16.4
12 0.00 0.97 0.00 2203 20.8 11.1 110.5
13 0.00 0.00 -0.97 2243 20.8 9.9 112.7
14 0.00 0.00 0.97 1791 2.0 0.5 8.2
15 0.00 0.00 0.00 2154 21.0 10.1 102.3
16 0.00 0.00 0.00 2161 18.0 7.8 96.1
17 0.00 0.00 0.00 2192 21.9 10.2 104.0
18 0.00 0.00 0.00 2150 19.3 10.7 85.7
19 0.00 0.00 0.00 2174 19.6 9.9 100.7
20 0.00 0.00 0.00 2160 18.6 8.0 88.2

Table 2. Material Model of Polyester Fly Ash Polymer Concrete

Regression Model according to property

coefficient Flexural strength Tensile strength Compress. strength
A0 19.68 9.47 96.03
A1 -3.11 -0.61 -22.48
A2 6.21 2.86 29.70
A3 -10.82 -4.90 -63.03
A11 -2.98 -0.62 -17.15
A22 -7.34 -2.96 -32.56
A33 -7.98 -4.82 -35.75
A12 -2.56 -0.33 -9.14
A13 -3.23 -3.46 -17.24
A23 9.18 4.05 27.13
Correlation 0.97 0.96 0.95
coeff.
The Wages and Sufficient Ranges of Properties for 3 Considered Variants

Property Variant I Variant II Variant III Sufficient range

Flexural strength, MPa 0.45 0.20 0.70 20 ÷ 30
Compressive strength, MPa 0.45 0.70 0.20 85 ÷ 95
Density, kg/m3 0.10 0.10 0.10 6 ÷ 12

a) b)

Compressive strength [MPa]

Compressive strength [MPa]

A/B Ash/M
B/M
A/B

c) d)
Flexural strength [MPa]

Tensile strength [MPa]

B/M Ash/M
B/M Ash/M

>1
<1
<7
<5
Fig. 5. Graphical Representation of the Material Model: a – Compressive <2

Strength in Function of A/B and B/M; b – Compressive Strength in Function of

Variables A/B and Ash/M; c – Flexural Strength; d – Tensile Strength; Both in
Function of B/M and Ash/M
In the second variant wage of compressive strength was higher (0.70) than wage of flexural
strength (0.20) and in the third variant it was opposite. All variants concerned polymer
concrete as a material of pre-cast elements that work under compressive loads. In the third
case it was assumed that the elements were also exposed to bending loads.

On the base of given above wages and sufficient ranges (see Table 3) overall desirability for
all polymer concretes designed and tested according to used statistical design was calculated
(Table 4). Taking into account that satisfactory level of overall desirability is 0.37 [Czarnecki
et all. 1999] the great majority of the PC compositions containing up to 50% of calcium fly
ash were evaluated as useful towards demanded criteria (bolded values). Using the values of
overall desirability for the particular concretes for each variant the regression functions which
describe the relations between the overall desirability and the material parameters were
evaluated. These functions were treated as an advanced material model. The regression
functions were described by the second degree polynomials – compare equation (1) – and the
values of the regression coefficients are presented in Table 5. Graphical representation of
advanced material model is presented on Fig. 6.

RESULTS AND DISCUSSIONS

The first part of the paper, where the influence of calcium fly ashes on polyester resin setting
process was evaluated, showed that although the applied microfillers presented differences in
granulometric composition, the typical PC microfiller – quartzite meal and calcium fly ash of
brown coal showed similar influence on hardening process – similar character of changes:
rapid drop of temperature of hardening along with increase of gel time. The calcium fly ash
of hard coal showed different influence: the drop of temperature of hardening was
comparable but in much wider range of variability of gel time, which correspond with
relation: hardening temperature – hardening time (as hardening time and gel time are strongly
correlated). Moreover, the analysis of tests results showed that exceeding value of 0.75 of
relative content of calcium fly ash of hard coal caused decrease of relative conductivity to
30% what meant that such mix had very low workability in comparison to other mixes.

In the second part of the paper there was presented the material models (basic and advanced)
of polyester concrete containing calcium fly ash of hard coal which make possible to
determine relations between the ingredients and the mechanical parameters of PC and
evaluate how the particular content of calcium fly ash influence on the mechanical strength.

The analysis of the basic material model, as well as overall desirability function, indicated
that the calcium fly ash content in the microfiller due to compressive strength should not
exceed 50% – this value appears to be proper limit for the relatively high use of utilized
calcium fly ash, satisfactory values of compressive strength and relatively good workability,
which gets worse with an increase in the quantity of calcium fly ash in the microfiller.
Analysis of data from the bending and tensile tests confirmed the above findings: content of
the calcium fly ash should not exceed 50%. Higher content caused significant decrease of the
workability and in consequence improper compaction of the mix. As a result the mechanical
properties decreased and the results scatter increased – the differences reached up to 80% in
value for samples of the fly ash content of between 79.5 and 98.5%. However the 50%
calcium fly ash content in is quite a high content and certainly confirms the validity of studies
using calcium fly ashes in polymer concretes as microfillers. The influence of calcium fly ash
presence on density of concretes was not very strong.
Table 4. Overall Desirability for All Tested Fly Ash PC for 3 Considered
Variants

No Material variables Overall desirability

X1 (A/B) X2 (B/M) X3 (Ash/M) Variant Variant Variant
coded (real) coded (real) coded (real) I II III
1 -0.58 (6.050) -0.58 (0.442) -0.58 (0.210) 0.81 0.90 0.66
2 (real)
0.58 (8.950) -0.58 (real)
(0.442) -0.58 (real)
(0.210) 0.68 0.78 0.56
3 -0.58 (6.050) 0.58 (0.558) -0.58 (0.210) 0.70 0.81 0.55
4 -0.58 (6.050) -0.58 (0.442) 0.58 (0.790) 0.00 0.00 0.00
5 0.58 (8.950) 0.58 (0.558) -0.58 (0.210) 0.80 0.90 0.64
6 0.58 (8.950) -0.58 (0.442) 0.58 (0.790) 0.00 0.00 0.00
7 -0.58 (6.050) 0.58 (0.558) 0.58 (0.790) 0.14 0.07 0.23
8 0.58 (8.950) 0.58 (0.558) 0.58 (0.790) 0.00 0.00 0.00
9 -0.97 (5.075) 0.00 (0.500) 0.00 (0.500) 0.79 0.90 0.62
10 0.97 (9.925) 0.00 (0.500) 0.00 (0.500) 0.00 0.00 0.02
11 0.00 (7.500) -0.97 (0.403) 0.00 (0.500) 0.00 0.00 0.00
12 0.00 (7.500) 0.97 (0.597) 0.00 (0.500) 0.77 0.87 0.61
13 0.00 (7.500) 0.00 (0.500) -0.97 (0.015) 0.79 0.80 0.63
14 0.00 (7.500) 0.00 (0.500) 0.97 (0.985) 0.00 0.00 0.00
15 0.00 (7.500) 0.00 (0.500) 0.00 (0.500) 0.68 0.77 0.56
16 0.00 (7.500) 0.00 (0.500) 0.00 (0.500 0.56 0.66 0.45
17 0.00 (7.500) 0.00 (0.500) 0.00 (0.500) 0.71 0.80 0.60
18 0.00 (7.500) 0.00 (0.500) 0.00 (0.500) 0.41 0.43 0.40
19 0.00 (7.500) 0.00 (0.500) 0.00 (0.500) 0.66 0.75 0.52
20 0.00 (7.500) 0.00 (0.500) 0.00 (0.500) 0.46 0.49 0.40

Table 5. Advanced Material Model of Fly Ash Polymer Concrete – Overall

Desirability in Function of the Properties Values

Regression Values of regression coefficient for

coefficient overall desirability regression function
Variant I Variant II Variant III
A0 0.58 0.65 0.49
A1 -0.19 -0.20 -0.16
A2 0.18 0.20 0.16
A3 -0.53 -0.61 -0.41
A11 -0.18 -0.21 -0.16
A22 -0.20 -0.22 -0.17
A33 -0.18 -0.21 -0.16
A12 0.03 0.05 -0.01
A13 -0.04 -0.02 -0.08
A23 0.05 0.02 0.10
Correlation 0.89 0.885 0.91
coeff.
a)

Overall desirability
Overall desirability

Ash/M
B/M
A/B Ash/M

b)
Overall desirability

Overall desirability

Ash/M
A/B B/M Ash/M

c)
Overall desirability

Overall desirability

B/M
Ash/M Ash/M
A/B

Fig. 6. Graphical Representation of Overall Desirability Function vs. Material

Variables: A/B and Ash/M (left) and B/M and Ash/M (right): a- Variant I;
b – Variant II; c – Variant III.
 CONCLUSIONS

The following conclusions can be formulated from the investigation presented in the paper:
The analysis of tests results has shown, that replacing typical microfiller with calcium fly
ash from coal combustion in polymer concrete mix is possible but in limited range – up
to 50% due significant decrease of mix workability.
The mechanical properties (flexural, tensile, compressive strength) of polymer concrete
containing more than 50% calcium fly ash in microfiller decrease significantly.
Calcium fly ash of hard coal causes extending gel and hardening time of polyester resin
in comparison to quartzite meal and calcium fly ash of brown coal.
Calcium fly ash of brown coal shows similar influence on hardening process as quartzite
meal, the typical PC microfiller.

ACKNOWLEDGEMENTS

This work has been done in the framework of project granted by Polish Ministry of Science
and High Education - grant number N N506 371434. The authors are thankful to Maciej
Bratek for carrying out the tests of hardening process of polyester binders which were done at
the Department of Building Materials Engineering.

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